Small, volatile carbosilanes containing only carbon, hydrogen and silicon with a carbon to silicon ratio of between 2:1 and 1:2 have been shown to be excellent precursors for the deposition of silicon carbide films in microelectronic applications. Typically, the term “small carbosilane” refers to compounds containing up to about nine backbone (silicon and/or carbon) atoms. Conventional syntheses of these low molecular weight (up to about 300 Daltons) carbosilanes include ‘in-situ’ Grignard approaches, which invariably result in the production of a vast mixture of products, including polymeric materials. It has proven very difficult to isolate pure materials from these reaction mixtures in any useful quantities. Another conventional approach to small carbosilanes involves generating silylenes in the presence of compounds containing silicon-hydrogen bonds to effect the insertion of the silylene into the Si—H bond. However, this method, upon reduction, also yields a mixture of products, including 1,1,1,3,3,3-disilapropane as a major product. Accordingly, superior methods for preparing small carbosilanes in useful quantities would be desirable.